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Chemical Structure| 26116-12-1 Chemical Structure| 26116-12-1
Chemical Structure| 26116-12-1

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Product Details of Sulpiride impurity A

CAS No. :26116-12-1
Formula : C7H16N2
M.W : 128.22
SMILES Code : CCN1CCCC1CN
MDL No. :MFCD00003178
InChI Key :UNRBEYYLYRXYCG-UHFFFAOYSA-N
Pubchem ID :117295

Safety of Sulpiride impurity A

GHS Pictogram:
Signal Word:Danger
Hazard Statements:H225-H314
Precautionary Statements:P280-P305+P351+P338-P310
Class:3(8)
UN#:2733
Packing Group:

Application In Synthesis of Sulpiride impurity A

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 26116-12-1 ]

[ 26116-12-1 ] Synthesis Path-Downstream   1~6

  • 1
  • [ 26116-12-1 ]
  • [ 19641-29-3 ]
  • 6-Chloro-2-(1-ethyl-pyrrolidin-2-ylmethyl)-2,3-dihydro-isoindol-1-one [ No CAS ]
  • 2
  • [ 26116-12-1 ]
  • [ 72411-89-3 ]
  • [ 72412-44-3 ]
  • 3
  • [ 498-63-5 ]
  • [ 26116-12-1 ]
  • 4
  • [ 26116-12-1 ]
  • [ 71675-87-1 ]
  • [ 541-41-3 ]
  • [ 71675-85-9 ]
YieldReaction ConditionsOperation in experiment
61% With triethylamine; In water; acetone; N-(1-ethyl 2-pyrrolidylmethyl) 2-methoxy 4-amino 5-ethylsulphonyl benzamide 81 g of <strong>[71675-87-1]2-methoxy 4-amino 5-ethylsulphonyl benzoic acid</strong> and 297 cm3 of acetone are placed in a flask fitted with an agitator, a thermometer and a dropping funnel, followed by 33 g of triethylamine. The solution is cooled to 0° C., then 30 g of ethyl chloroformate is added drop by drop between 0° and 5° C. When the mixture has been agitated 51 g of 1-ethyl 2-amino methyl pyrrolidine is added drop by drop between 5° and 10° C. The mixture is agitated at 10° C. then at ambient temperature. The triethylamine hydrochloride which precipitates is drained, then the acetone is distilled. The residue is dissolved in 600 cm3 of water in the presence of caustic soda solution. The base crystallises after seeding and is drained, washed with water and dried. When the crystals have been purified by passing them through hydrochloride and re-crystallising them in acetone, 66 g of N-[1-ethyl 2-pyrrolidylmethyl] 2-methoxy 4-amino 5-ethylsulphonyl benzamide is obtained (yield 61percent-M.P.=126° to 127° C.).
  • 5
  • [ 26116-12-1 ]
  • [ 71675-87-1 ]
  • [ 71675-85-9 ]
YieldReaction ConditionsOperation in experiment
70% With chloroformic acid ethyl ester; triethylamine; In acetone; at 0 - 30℃; To a stirring mixture of 4-amino-2-methoxy-5 -ethyl sulphonyl benzoic acid (IV) and acetone (5.0 L) at 0-5°C, triethyl amine (0.405 Kg) was added and stirred followed by addition of ethyl chloroformate (0.368 Kg). N-ethyl-2-amino methyl pyrrolidine (0.627 Kg) was added to the reaction mass at 5-10°C. Temperature of reaction mass was raised to 25-30°C and stirred for 120 min. To the same reaction mass triethyl amine (0.405 Kg) and ethyl chloroformate (0.368 Kg) was added with maintaining the temperature. Reaction mass was stirred for 120 min. After completion of reaction, water (4.0 L) was added. Reaction mass was filtered and washed with water (2.0 L). Filtrate was collected and water was added (9.0 L). pH of the reaction mass was adjusted to 10.8-1 1.2 by using 20percent NaOH solution. Reaction mass was stirred for 240-300 min, filtered and washed with water. Solid was dried under vacuumYield : 70percentPurity: 98percent
  • 6
  • [ 26116-12-1 ]
  • [ 33045-53-3 ]
  • [ 15676-16-1 ]
YieldReaction ConditionsOperation in experiment
88.5% In glycerol; at 110 - 120℃; for 4.0h; 25.9 g of <strong>[33045-53-3]ethyl 2-methoxy-5-sulfamoylbenzoate</strong>,1-ethyl-2-aminomethyltetrahydropyrrolidine 15g and glycerol 20g were added to the reaction flask,The reaction was carried out at 110-120 ° C for 4 hours, the reaction was completed, and it was cooled to 80 ° C.Add 40g of ethanol and stir for 10 minutes.Cool to 5 ° C and stir for 1 hour, filter,It was washed with ethanol and dried at 65 °C. The yield was 88.5percent and the purity was 99.5percent.
 

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